Simultaneous determination of cadmium, lead and copper in chocolate samples by square wave anodic stripping voltammetry.

In this work, an effective and simple method is proposed for the simultaneous determination of cadmium, lead and copper in chocolate samples by Square Wave Anodic Stripping Voltammetry (SWASV). An ultrasonic bath was used for the extraction of cadmium, lead and copper from fourteen chocolate samples using HNO3 solution (7 mol L-1). The electrochemical system consisted of a cell with three electrodes and HCl solution (10 mmol L-1) as the supporting electrolyte. An efficient extraction of the metals (~100%) was attained after 1 h of ultrasonic pre-treatment. Quantitative analysis was carried out by the standard addition method. Good linearity, precision and accuracy were obtained in the range of concentrations examined. The accuracy was evaluated by means of a reference sample of spiked skim milk powder (BCR 151) to prove the reliability of the method. Detection limits (LOD) of 0.089, 0.059 and 0.018 µg g-1 were found for cadmium, copper and lead, respectively, in the chocolate samples. Concentrations in chocolate samples were 4.30-138 µg g-1 for Cu and 0.83-27.9 µg g-1 for Pb, with no significant Cd. The simultaneous determination brings advantages to other methods already reported for chocolate analysis and the samples preparation proposed avoids the traditional sample mineralization step. These characteristics show this new method is especially attractive for case studies and routine analysis.

Direct analysis of ascorbic acid in food beverage samples by flow injection analysis using reduced graphene oxide sensor.

In this paper, a simple, sensitive and precise electroanalytical method was developed using flow injection analysis (FIA) with amperometric detection and reduced graphene oxide sensor for ascorbic acid determination in samples of multivitamin beverages, milk, fermented milk, and milk chocolate. The advantages of this sensor include a potential displacement of 450 mV and a 2-fold peak current increase for electrochemical oxidation of ascorbic acid, which resulted in a highly sensitive method. No interference of sample matrix was observed, avoiding solvent extraction procedures (samples were only diluted). The FIA allowed a high analytical frequency, approximately 96 injections per hour, together with adequate detection limit of 4.7 µmol L-1. Good precision (RSD < 7%) and accuracy (recoveries between 91 and 108%) evidenced the robustness of the method. The method was compared with ultra-fast liquid chromatography (UFLC) obtaining statistically similar results (95% confidence level). The ascorbic acid content in samples varied from 0.065 to 2.53 mmol L-1.

Chromium Levels in Tobacco, Filter and Ash of Illicit Brands Cigarettes Marketed in Brazil.

Smoking is a public health problem and an important source of exposure to toxic metals. This work describes an efficient analytical method comparable to the ones based on atomic emission techniques for the determination of chromium in different constituent parts of cigarette samples (tobacco, filters and ashes) using electrothermal vaporization-atomic absorption spectrometry. The method was evaluated using 12 samples, and the results showed recovery values between 83 and 107%. The accuracy was also evaluated using a reference sample of tomato leaves (NIST SRM 1573a), which proved the efficiency of the method. The limits of detection of the developed method were 20.4, 75.8 and 80.7 ng g-1 for tobacco, filter and cigarette ash samples, respectively. The average chromium values found for the analyzed samples were in the range of 0.96 to 3.85 and from 0.32 to 0.80 µg/cigarette for tobacco and ashes, respectively. For most pre-burn and post-burn filter samples, the values of chromium concentration remained below limits of detection. The developed method presented adequate results about precision and accuracy, demonstrating its applicability in the determination of chromium in cigarette samples.

Selenium Content in the Liver of Wistar Rats Fed Diets of Different Fatty Acid Quality.

The purpose of this work was to measure the amounts of selected mineral elements (sodium, calcium, iron, selenium, magnesium, zinc, copper, and manganese) in the liver of Wistar rats and evaluate possible correlations between the levels of these minerals and the lipid metabolism in the studied animals. Three experimental groups each containing six Wistar rats were designed. Each group was fed a different diet. The control group was fed a diet prepared with fresh soybean oil and named control group--CG. The second group (named experimental group B--EGB) and third group (named experimental group C--EGC) were fed a diet containing soybean oil that had been used to fry different foods for four or ten cycles, respectively. The mineral elements in Wistar rat livers were measured by inductively coupled plasma optical emission spectrometry (ICP OES). Only the elements calcium and selenium differed significantly between the control and experimental groups. There was a significant reduction of 33% for Ca and 41% for Se in the EGB in comparison to the control group. The reduction in mineral concentration, especially Se, is the result of interactions with fatty acid metabolism. The animals in the EGC exhibited more intracytoplasmic accumulation of fat and more intense vasodilatation, in relation to the other groups. Collectively, evidence hereby collected suggests that impaired dietary lipid quality in otherwise balanced diets can reduce hepatic Se levels and potentially harm liver function.

Lead biomonitoring in different organs of lead intoxicated rats employing GF AAS and different sample preparations.

An analytical procedure was developed for the determination of lead in different tissues from Wistar Hanover rats, previously intoxicated with lead acetate during a toxicological study. About 25 mg of dried sample (bone, liver, kidney, heart, lung and spleen) were mixed with 8.0 mL of 7.00 mol L(-1) nitric acid and digested using microwave radiation in closed vessel. Except for the bone samples, the other tissues could also be analyzed after alkaline solubilization with TMAH. All the digested or solubilized samples were analyzed by graphite furnace atomic absorption spectrometry. Good accuracy and precision were attained when analyzing reference standard materials (for bone, liver and kidney) and also from addition to recovery experiments (for heart, lung and spleen tissues). The method was applied to samples from nine animals and the results suggested that there is a profile for lead bioaccumulation in these animals, which seemed to adapt themselves to continuous lead exposure.